反応 #44518

ord-6c9f9b57843d4fe9a20c843dfd7e6fce

溶媒

反応条件

温度
60°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    抽出subjected to extraction with ethyl acetate
  2. 2
    workup.ADDITIONThen water was added
  3. 3
    抽出the mixture was subjected to extraction with ethyl acetate
  4. 4
    洗浄The organic layer was washed with water and brine sequentially
  5. 5
    乾燥dried over anhydrous Na2SO4
  6. 6
    濃縮concentrated
  7. 7
    その他The resulting residue was purified by column chromatography

実験手順

6-(2-chloropyrimidin-4-yloxy)-N,2-dimethylbenzofuran-3-carboxamide (0.1 mmol) and 3-methoxyaniline (0.1 mmol) were dissolved in 0.5 ml DMF. To this was added p-TsOH monohydrate (0.2 mmol). The reaction mixture was stirred at 60° C. for 5 hours, and subjected to extraction with ethyl acetate. Then water was added and the mixture was subjected to extraction with ethyl acetate. The organic layer was washed with water and brine sequentially, dried over anhydrous Na2SO4, and concentrated. The resulting residue was purified by column chromatography to provide the title product in a yield of 80%.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US07737157B2uspto-grants-2010_06